Cerenano Presentation

Using Renewable Nanotechnology
(and Other Novel Approaches) to
Improve Base Paper Performance
Robert Hamilton
President
Stirling Consulting, Inc.
AWA Conferences & Events
AWA Silicone Technology Seminar 2014
March 19, 2014
Park Plaza Hotel Amsterdam Airport
Amsterdam, Netherlands
Background
CNF Developments at the
University of Maine
2
Cellulose Nanofibrils (CNF)
The Renewable Nanomaterial
•  CNF can be made from any plant matter.
ü Process uses a series of mechanical refining steps.
ü Resulting material is FDA compliant and compatible
with any aqueous system. CNF is cellulose.
•  Not to be confused with Cellulose NanoCrystals
(CNC)
ü Produced using more expensive strong acid
hydrolysis process.
3
Papermaking Fiber Compared to
Cellulose Nanofibrils
Wood Cellulose Papermaking Fiber
Diameter of 15 to 40 microns
Cellulose Nanofibrils
Diameter of 0.02 microns
4
University of Maine CNF Project History
•  1990’s – University of Maine begins development of a
process to produce cellulose nanofibrils (CNF).
•  Cost effective process enables consideration of paper
applications
–  Wet end addition
–  Coating applications
•  The University of Maine joins research consortium led by
USDA’s Forest Products Laboratory to support
commercialization of renewable nanomaterials.
•  Initial research demonstrates potential of nanofibrillated
cellulose in paper applications.
ü  Tighter sheet
ü  More uniform surface
ü  Better printability
ü  Reduced opacity
ü  Reduced energy requirements
5
Cellulose Nanofibrils
FE-SEM images of UMaine CNF
X 100k 200 nm
CNFwidth ~20 nm
X 300k University of Maine
Process Development Center
100 nm
6
University of Maine Proprietary
Cellulose Nanofibril Process
•  Novel method to produce CNF
–  High performance additive
•  Wide range of applications
•  One current focus is release base
–  Low cost
–  Commercially scalable
–  Patent pending technology
7
CNF Production - Process Flow
Current Pilot Plant Sytem 300 lbs/day Chem Treatment
F
Wood Pulp
Refiner feed
Chest
Storage Chest
Side Agitator
Pulper
HeatX
13" & 20" refiner
8
Maximizing Holdout, Smoothness & Strength
Cerenano (CN) Process Flow
CNF
Cooked Starch
Chemical
Treatment
Steam
Blending
(with good
mixing)
CN to Machine System
9
Novel Release Base Project
Phase 1 – Wet End Development
10
CNF Release Base Project History
August 2013 to October 2013
Runs on commercial
equipment – lightweight
base & 3.2 mil
March 2012
Project funded by
Maine Technology
Institute
October 2013 to March 2014
Start Phase 2
size press formulation
development & plans for
commercial trial work
Fall 2011
UMaine & Stirling
initiate novel
release base
project
April 2012 to July 2013
Lab & pilot studies
completed.
Patent application
filed.
11
Novel Release Base Project
• 
Project Objectives
ü  Utilizing CNF and other U Maine proprietary
technologies, design a novel release base paper
that:
1.  Reduces silicone coating demand through better holdout
and a more level sheet surface.
2.  Improves adhesive transfer with a more level sheet surface
(more film-like performance).
3.  Improves sheet strength that enables reducing basis
weight and caliper.
4.  Has better dimensional and thermal stability.
5.  Lowers energy requirements for refining and drying.
12
Novel Release Base Project, cont’d
•  Phase 1 Project Steps
ü Benchmarking current commercial products
ü Lab evaluations of various furnishes
ü Pilot paper machine runs on most promising
furnish
ü Initial commercial scale-up (small machine)
•  Status: Complete
13
Results - Handsheet Evaluations
•  Comparing the same fiber furnish at different
refining levels (moderate vs. glassine level), the
sheets with novel CNF or CN content were:
ü More dense
ü Much higher in Gurley Porosity
ü Much lower in PPS (S-10)
ü Much lower in shrinkage
ü Similar in opacity
ü Similar in tensile but somewhat lower in tear
•  CN furnishes showed the best results
14
University of Maine Pilot Paper Machine
Trim = 13 in. (33 cm)
Speed Range = 10 to 160 fpm (3 to 49 m/min.)
Basis Weight Range = 15.5 to 140 lb./3,000 ft.2 (25 to 225 gsm)
State of the art gauging and control systems
15
Pilot Paper Machine Trial Conditions & Results
•  Conditions
ü  80 gsm base, 70% NBHK, 30% NBSK fiber furnish
ü  2 controls (100 & 200 HB CSF, CN 200 @ 200 CSF
ü  Soft nip calendered with no size press treatment and two different size
press treatments (standard & novel)
•  Machine operation.
ü  Drainage rate
o  CN condition slightly slower than 200 CSF control
o  CN condition much faster than 100 CSF control
ü  Drying
o  CN condition 0.5% lower moisture than 100 CSF control
ü  CD shrinkage
o  CN condition higher than 200 CSF control
o  CN condition less than 100 CSF control
•  Results
ü  Handsheet findings confirmed qualitatively – 2.9 X Gurley and
approximately 1% less shrinkage, for example
16
Si Coating of Pilot Machine Trial
Conclusions
•  CN 200 untreated base performed better than
expected regarding Si holdout compared to the
untreated control.
•  Size press treated CN bases also out performed
size press treated control, but not by as great a
margin. More work on size press formulation
needed. (Project Phase 2)
•  Ready to scale-up wet end application of CN to
a small commercial machine.
17
Commercial Scale-up Objectives
•  First Trial
ü Run lightweight base without size press treatment to
verify performance of prototype base at a lighter basis
weight.
ü Target MF/MG direct Si coating base applications.
•  Second Trial
ü Run standard 3.2 mil densified kraft sheet (for label/
tape and other applications) with commercial size
press application.
ü Run conventional size press starch on both control
and novel base as lab development of novel size
press formula not complete.
18
Scale-up Machine Location
Turners Falls, Massachusetts, USA
• 
• 
• 
• 
• 
• 
• 
• 
• 
Extensive refining capability
108” fourdrinier (max. trim)
Conventional press section (1st & 2nd)
Conventional dryers
Breaker stack (not used)
Tub size press
Hot, soft calender (1 nip per side)
Basis weight capability down to 28 lb./3,000 ft.² (45 gsm)
Good formation
19
Scale-up
Operational Conditions - Lightweight
•  Run on August 29, 2013
•  Target basis weight of 28 lb. (approx. 45 gsm)
•  50% Bleached Southern Softwood/50% Bleached
Northern Hardwood furnish
•  300 CSF HB freeness
•  Neutral pH (could be run either acid or alkaline)
•  No filler, no internal size
•  No size press
•  Hot soft calender – one nip per side – 1,800 pli, 180°F
•  Added Cerenano material at 200 lb./ton (100 kg/tonne)
finished paper for trial condition CN200 at blend chest –
no other furnish or machine condition changes
20
Scale-up
Lightweight Trial Results – Operational Summary
•  Ran approximately 1.5 hours after adding Cerenano with
no breaks and no operating issues
•  Observations:
ü Dry line moved one flat box toward the couch.
ü Couch vacuum increased by 20%.
ü Minimal operational adjustments – took out some water
and increased flat box vacuum to reposition the dry line.
ü Sheet moisture went from 2.4% to 5.2% with no
operational issues and no roll condition issues.
ü Bone dry basis weight increased by around 9%.
21
Commercial Machine Scale-up - Lightweight
Weight/Density Quality Summary - Conditioned Tests*
30
28
26
24
22
20
18
16
14
12
10
8
6
4
2
0
26.7
28.2
22.0
20.0
13.0
Basis Wt. (#/3000)
Caliper (mils x 10)
Control
14.8
Density (Bs.Wt,/Cal.)
CN200
* Not corrected for basis weight difference
22
Commercial Machine Scale-up - Lightweight
Strength Quality Summary - Conditioned Tests*
35
33
31
29
27
25
23
21
19
17
15
13
11
9
7
5
3
1
-1
26.60
30.50
32.20
31.30
20.40
8.49
Burst (psi)
CD Tear Index
Control
10.37
MD Tensile
Index/10
3.20
Internal Bond/10
CN200
* Not corrected for basis weight difference
23
Commercial Machine Scale-up - Lightweight
Porosity & Surface Quality Summary - Conditioned Tests*
70
60
50
40
66.7
30
52.0
20
10
0
8.1
Porosity
(sec./10)
14.4
8.5
Sheff. Sm. Top
(SU/10)
12.9
42.0
39.0
8.6
Sheff. Sm.
Wire (SU/10)
Control
48.0
PPS Top (x10) PPS Wire (x10)
CN200
* Not corrected for basis weight difference
24
A Look at the Sheet’s Surface
Control – 208 X
CN 200 – 245 X
25
(An Unfair) Comparison to a Commercial
Glassine Sheet
X 131
X 121
CN 200
No Size Press Treatment & Soft Nip
Commercial Glassine
•  29.5 # Basis Weight
•  2.0 mil, 14.8 #/mil Density
•  667 sec. Gurley Porosity
•  Sheffield - 85/86
•  PPS – 3.9/4.2
•  CD Tear Index – 20.4
•  MD Tensile Index – 103.7
•  42.5 # Basis Weight
•  2.2 mil, 19.3 #/mil Density
•  10.700 sec. Gurley Porosity
•  Sheffield – 32/74
•  PPS – 1.7/2.0
•  CD Tear Index – 6.1
• MD Tensile Index – 105.9
26
Scale-up
Operational Conditions – 3.2 Mil
•  Run on October 17, 2013
•  Target basis weight of 52 lb. (approx. 85 gsm)
•  50% Bleached Southern Softwood/50% Bleached
Northern Hardwood furnish
•  300 CSF HB freeness
•  Neutral pH (could be run either acid or alkaline)
•  No filler, no internal size
•  Starch size press treatment
•  Hot soft calender – one nip per side – 1,800 pli, 180°F
•  Added Cerenano material at 200 lb./ton (100 kg/tonne)
finished paper for trial condition CN200 at blend chest –
no other furnish or machine condition changes
27
Scale-up
3.2 Mil Trial Results – Operational Summary
•  Ran approximately 2 hours after adding Cerenano with
no breaks and no operating issues
•  Observations:
ü Wet end operation as with the lightweight trial, with couch
vacuum increasing and dry line moving down the table.
ü Similar wet end adjustments as with the lightweight trial.
ü Size press pickup minimal
ü Density development was less than with the lightweight,
and it was concluded that the soft nip calender was not
capable of adequate loading to densify adequately at this
basis weight.
28
Commercial Machine Scale-up – 3.2 Mil
Weight/Density Quality Summary - Conditioned Tests*
55
50
45
40
35
30
25
52.3
52.2
20
36.0
15
10
35.0
14.5
5
14.9
0
Basis Wt. (#/3000)
Caliper (mils x 10)
Control
Density (Bs.Wt,/Cal.)
CN200
* Not corrected for basis weight difference
29
Commercial Machine Scale-up – 3.2 Mil
Strength Quality Summary - Conditioned Tests*
55
50
45
40
35
30
25
20
51.0
43.0
43.1
49.8
34.2
15
10
5
9.1
13.9
7.8
0
Burst (psi)
CD Tear Index
Control
MD Tensile Index
Internal Bond/10
CN200
* Not corrected for basis weight difference
30
Commercial Machine Scale-up – 3.2 Mil
Porosity & Surface Quality Summary - Conditioned Tests*
24
22
20
18
16
14
12
10
8
6
4
2
0
23.1
9.2
9.6
9.0
9.5
4.3
Porosity
(sec./10)
3.7
3.7
3.7
4.1
Sheff. Sm. Top Sheff. Sm. Wire PPS Top (S-10 - PPS Wire (S-10
(SU/10)
(SU/10)
µm)
-µm)
Control
CN 200
* Not corrected for basis weight difference
31
Conclusions – Commercial Trials
•  The lightweight trial:
ü  increased sheet density (14%)
ü  significant improvement in internal bond (906%) and some improvement in
tensile (22%) and burst (15%)
ü  loss in tear index (-35%)
ü  significantly less air permeability (723% increase in Gurley seconds)
ü  notably improved surface as shown by Sheffield, PPS and SEM evaluations
ü  no operational issues
•  The 3.2 mil trial:
ü  slight increase in sheet density (3%), a result of soft nip capability
ü  significant improvement in internal bond (146%) but mush less dramatic
than for the lightweight
ü  improvements in tensile (16%) and burst (19%), similar order of magnitude
compared to the lightweight
ü  loss in tear index (-15%), less than the lightweight
ü  significantly less air permeability (437% increase in Gurley seconds)
ü  little difference in surface properties as a result of calender capability at this
basis weight
ü  No operational issues
32
Developmental Issues Remaining
•  Lightweight:
ü complete evaluation of pilot silicone coating
(solventless thermal cure)
ü emulsion silicone coating evaluation
ü end use evaluations (hand peel, baking)
•  3.2 mil
ü develop an improved size press formulation
ü trial run with novel size press formula and better
calendering capability
ü pilot silicone coating and end use evaluations for SCK
and CCK applications
33
Novel Release Base Project
Phase 2 – Size Press Development
34
Novel Release Base Project, Phase 2
•  Size Press Formula Development Objectives:
ü Reduction of silicone coating usage
ü Improved sheet dimensional stability
ü Use of renewable resource based materials
ü Reduction in energy consumption
ü Ability to apply in conventional size presses,
metering size presses, blade or rod coaters
35
Novel Release Base Project, Phase 2 cont’d
•  Size Press Formulation Development
ü  Define specific project approach – surface treatment
formulation
1)  Develop high solids formulations with appropriate rheology
for operation with conventional and/or high speed metering
size presses or blade/rod coaters.
2)  A conventional size press formulation used as a control.
3)  Evaluate using base paper produced in August 2013
commercial base paper scale-up trial on the University of
Maine’s pilot coater (blade configuration).
•  Bench and initial pilot work completed in
December 2013/January 2014
36
University of Maine Pilot Coater
Maximum Trim = 12 in. (30.5 cm)
Maximum Speed = 100 fpm (30 m/min.)
Capability to simulate many coating application methods,
including blade and rod coaters.
37
Pilot Size Press Formula & Conditions
Condition
Control
Novel
Modified PLA (proprietary)
n/a
90% by
weight
Food grade talc (can be platey clay)
n/a
10% by
weight
100% by
weight
n/a
25%
78%
Low Shear Viscosity
n/a
200 cps
Surface Size/Coating Pickup (gsm)
3.2
4.3 & 8.8
Blade
Blade
Components
Ethylated Starch
Rheological Characteristics & Pickup
Solids
Coater Configuration
38
Results
12.0
11.5
11.0
10.5
10.0
9.5
9.0
8.5
8.0
7.5
7.0
6.5
6.0
5.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
0.0
12.0
10.0
6.2
4.8
0.081
3.0
2.6
0.63
3.1
0.9
Gurley Porosity (sec./1,000)
Base 0/45.9
Novel 8.8/54.7
4.3
Control 3.2/49.1
Glassine -/64
1.4
PPS (S-10) Treated Side
Novel 4.3/50.2
Parchment (Baking)
39
Results, contd.
Starch 3.2 gsm 85 X
PLA 8.8 gsm 121 X
Base 85 X
PLA 4.3 gsm 107 X
Comm’l Glassine 121 X
40
Remaining Issues – Size Press/Coating
•  Improve cross linking to improve stability
and reduce tackiness seen on heavier
coat weight samples
•  Apply to 3.2 mil base
•  Evaluate effect of calendering on these
sheets – expected to further smooth the
sheet
•  Evaluate Si adhesion
41
Cost Analysis
42
Cerenano Cost Analysis
•  Cash Cost Components
o  Cellulose nanofibrils made from conventional papermaking wood
pulps
o  Pre-treatment chemical
o  Refining energy
o  Starch addition
•  Cash cost per ton of cellulose nanofibril additive (Cerenano)
approximates that of pulp used.
•  In addition, the CNF based additive will likely:
o  reduce total refining energy needed.
o  reduce softwood fiber required.
o  reduce drying energy requirements.
•  Therefore, finished base paper cost is projected to be at a par
with or possibly less than current release base papers.
•  Potential cost savings in ths finished release paper include
improved silicone coating coverage and reduce coat weight.
43
Relative Costs
102
% of Control Cost
101
100
99
98
97
96
100
101
95
96
94
93
95
92
Control
CN 200 - Reduced Softwood
CN 200 - Same Fiber Furnish
CN 200 - Minimal Softwood
44
Material Availability
45
•  CNF
ü  Available in lab and short run (pilot/small commercial) quantities
from U Maine’s Process Development Pilot Plant.
ü  A very low solids material, significantly reducing acceptable
shipping distances.
ü  Equipment to produce is commercially available (special refiner
plates).
ü  Capital requirements relatively low, plant footprint small and
manpower requirements minimal.
ü  Currently several parties with interest in producing in the North
East US.
•  PLA
ü  To date all produced in the laboratory.
ü  Industrial pilot plant scale-up imminent.
ü  Relatively simple process.
46
Commercialization
47
Status
•  Trial work on commercial equipment confirms lab and
pilot work regarding dramatic improvements in sheet
density, porosity, surface quality and Z-direction strength
(internal bond).
•  Evaluations continue, especially regarding size press
treatments and additional Si coating evaluations.
•  Commercial trials with CNF and CN for other
applications have demonstrated good operating
performance with similar quality improvements
•  Novel surface treatment formulations containing CNF
have been problematic regarding size pickup levels.
•  Modified PLA based formulations show great promise in
porosity and surface levelness development but need
fine tuning prior to a commercial trial.
48
Next Steps
•  Move forward with commercialization for lightweight
non-PS or hand peel applications (wet end addition)
•  For densified release applications:
ü Complete development of surface treatment formulations
using the novel PLA technology.
ü Determine optimum calendering levels for high density
release applications.
ü Generate prototypes with CNF content base and novel
surface treatment.
ü Verify potential to reduce silicone coating requirement and
validate commercial performance using commercial trial
product.
49
Thank you!
50

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